Designation D1856 − 09 (Reapproved 2015) Standard Test Method for Recovery of Asphalt From Solution by Abson Method1 This standard is issued under the fixed designation D1856; the number immediately f[.]
Trang 1Designation: D1856−09 (Reapproved 2015)
Standard Test Method for
This standard is issued under the fixed designation D1856; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision A number in parentheses indicates the year of last reapproval A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1 Scope
1.1 This test method covers the recovery by the Abson
method of asphalt from a solution from a previously conducted
extraction The asphalt is recovered with properties
substan-tially the same as those it possessed in the bituminous mixture
and in quantities sufficient for further testing
1.2 The values stated in SI units are to be regarded as the
standard The values given in parentheses are provided for
information only
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use It is the
responsibility of the user of this standard to establish
appro-priate safety and health practices and determine the
applica-bility of regulatory limitations prior to use.
2 Referenced Documents
2.1 ASTM Standards:2
C670Practice for Preparing Precision and Bias Statements
for Test Methods for Construction Materials
D2172Test Methods for Quantitative Extraction of Bitumen
From Bituminous Paving Mixtures
D2939Test Methods for Emulsified Bitumens Used as
Protective Coatings(Withdrawn 2012)3
D4080Specification for Trichloroethylene, Technical and
Vapor-Degreasing Grade
D6368Specification for Vapor-Degreasing Solvents Based
on Propyl Bromide and Technical Grade
normal-Propyl Bromide
E1Specification for ASTM Liquid-in-Glass Thermometers
3 Summary of Test Method
3.1 The solution of solvent and asphalt from an asphalt mix
extraction is distilled under prescribed conditions to a point
where most of the solvent has been distilled, at which time carbon dioxide gas is introduced into the distillation process to remove all traces of the extraction solvent The recovered asphalt (distillation residue) can then be subjected to further testing as required
4 Significance and Use
4.1 The asphalt should be extracted from the aggregate-asphalt mixture in accordance with Method A of Test Methods D2172 (centrifuge method) as there is some experimental evidence that the recovered asphalt may have slightly lower penetration values when recovered from solutions obtained from hot extraction methods
5 Apparatus
5.1 Centrifuge, batch unit capable of exerting a minimum
centrifugal force of 770 times gravity or continuous unit capable of exerting a minimum force of 3000 times gravity
5.2 Centrifuge Tubes—A supply of wide-mouth bottles or
centrifuge tubes may be used for the batch unit A tube as illustrated in Fig 1 has been found satisfactory for the continuous unit
5.3 Distillation Assembly, as shown inFig 2, and consisting
of the following items:
5.3.1 Extraction Flasks—Two 250-ml, wide-mouth,
heat-resistant flasks, one for distillation and the other for the receiver
5.3.2 Glass Tubing—Heat-resistant glass tubing, having
10-mm inside diameter and gooseneck shaped (as shown in Fig 2) for connecting the flask to the condenser
5.3.3 Inlet Aeration Tube,4at least 180 mm in length, having
a 6-mm outside diameter with a 10-mm bulb carrying six staggered side holes approximately 1.5 mm in diameter
5.3.4 Electric Heating Mantle, with variable transformer, oil
bath, or fluidized sand bath, to fit a 250-ml flask
5.3.5 Water-Jacketed Condenser, Allihn type, with 200-mm
minimum jacket length or equivalent
1 This method is under the jurisdiction of ASTM Committee D04 on Road and
Paving Materials and is the direct responsibility of Subcommittee D04.25 on
Analysis of Asphalt Mixtures.
Current edition approved Jan 1, 2015 Published February 2015 Originally
approved in 1961 Last previous edition approved in 2009 as D1856 – 09 DOI:
10.1520/D1856-09R15.
2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 The last approved version of this historical standard is referenced on
www.astm.org.
4 The sole source of supply of the apparatus known to the committee at this time
is Inlet Aeration Tube, Part No 226, available from Wm A Sales, Ltd., 419 Harvester Court, Wheeling, Ill 60090; request Part No 226 If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters Your comments will receive careful consideration at a meeting of the responsible technical committee, 1 which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959 United States
Trang 2FIG 1 Centrifuge Tube Example
FIG 2 Distillation Assembly for Bitumen Recovery
Trang 35.3.6 Thermometer—An ASTM Low Distillation
Thermom-eter 7E or 7F, as specified, having a range from −2 to 300°C or
30 to 580°F, respectively, and conforming to the requirements
in SpecificationE1
5.3.7 Gas Flowmeter,5as shown inFig 2, or any flowmeter
capable of indicating a gas flow of up to 1000 ml/min
5.3.8 Corks, No 20, drilled as shown inFig 2
5.3.9 Flexible Elastomeric Tubing, resistant to chlorinated
solvents having sufficient length and size to connect the
aeration tube to flowmeter, and equipped with a pinch clamp or
stopcock to close aeration tube prior to introducing carbon
dioxide
5.3.10 Separatory Funnel,6(Alternative Procedure, see
9.3.1) 125-ml capacity
6 Reagents and Materials
6.1 Carbon Dioxide Gas—A pressurized tank, with
pressure-reducing valve or other convenient source
6.2 Solvents
6.2.1 The solvent for extracting the asphalt from mixtures
may be trichloroethylene, conforming with Specification
D4080.7
6.2.2 The solvent for extracting the asphalt from mixtures
may be Normal Propyl Bromides (nPB) This solvent should
conform to Specification D6368.8
6.2.3 The solvent for extracting the asphalt from mixtures
may be reagent grade Methylene Chloride.8
7 Precautions
7.1 Warning—The solvent listed in 6.2 should be used only
under a hood or with an effective surface exhaust system in a
well-ventilated area, since they are toxic to various degrees
Consult the current Threshold Limit Concentration Committee
of the American Conference of Governmental Industrial
Hy-gienists for the current threshold limit values
7.2 These solvents in the presence of heat and moisture may
be hydrolyzed to form acids that are extremely corrosive to
certain metals, particularly when subject to contact over
lengthy periods of time Proper precautions should be taken to
not allow these solvents to remain in small quantities in the
effluent tanks of aluminum vacuum extractors
7.3 Exposure of these solvents or their vapors to high temperatures such as contact with flames, hot glowing surfaces,
or electric arcs can produce decomposition products such as hydrogen chloride Steel drums containing these solvents should be stored in a cool, dry location, kept tightly sealed, and opened as infrequently as possible The hydrogen chloride in decomposed solvent may harden an asphalt during the extrac-tion and recovery test
8 Sample
8.1 The sample shall consist of the solution from a previous extraction by Method A of Test Methods D2172 of asphalt-aggregate mixture of sufficient quantity to result in 75 to 100 g
of recovered bitumen More or less quantities of bitumen may
be recovered; however, the properties of the recovered bitumen may not be in agreement with those recovered of the afore-mentioned quantities, and in case of a disagreement, 75 to 100
g should be recovered
8.2 During the extraction process, it is important that all of the asphalt in the mixture be extracted as there could be some selective solvency of the asphalt and the harder, more viscous components of the asphalt might be left in the mixture if extraction is not carried to completion
8.3 Since heavy petroleum distillates such as mineral spirits
or kerosine will affect the properties of the recovered asphalt,
it is important to avoid the use of such solvents in cleaning the extraction and recovery apparatus and use only trichloroethyl-ene for cleaning Residues of heavy petroleum solvents on the equipment may contaminate the recovered asphalt and affect its test properties It is also necessary to use new filter rings, clean felt pads, or other uncontaminated filtering media in the extraction process to avoid contamination from a previous extraction
8.4 Generally, the bitumen in mixtures will progressively harden when exposed to air, particularly if the mixtures are in
a loose condition Therefore, it is important to protect bitumi-nous mixtures from exposure to air and preferably to store them in airtight containers at a temperature below 0°C (32°F) until they can be tested When samples of bituminous mixture are warmed for preparing representative proportions for extrac-tion tests in accordance with Method A of Test Methods D2172, they should be placed in an oven in covered containers and heated to a maximum temperature of 110°C (230°F) for the minimum time to obtain workability, but no longer than 30 min If the samples have been stored at a low temperature, they should be allowed to reach room temperature before placing them in the oven
9 Procedure
9.1 The entire procedure, from the start of the extraction to the final recovery, must be completed within 8 h
9.2 Centrifuge the solution from the previous extraction for
a minimum of 30 min at 770 times gravity in either bottles or centrifuge tubes in the specified batch apparatus If a continu-ous centrifuge is used, the extract solution shall be charged at
a rate not to exceed 150 ml/min, while the unit is operating at
5 The sole source of supply of the apparatus known to the committee at this time
is The Monostat Corp “Flowmeter” No 9144 If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
Your comments will receive careful consideration at a meeting of the responsible
technical committee, 1 which you may attend.
6 The sole source of supply of the apparatus known to the committee at this time
is Kimball separatory funnel No 29028 If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters Your
com-ments will receive careful consideration at a meeting of the responsible technical
committee, 1 which you may attend.
7 The sole source of supply of the apparatus known to the committee at this time
is American Conference of Governmental Industrial Hygienists, Inc (ACGIH),
1330 Kemper Meadow Dr., Cincinnati, OH 45240, (http://www.acgih.org) If you
are aware of alternative suppliers, please provide this information to ASTM
International Headquarters Your comments will receive careful consideration at a
meeting of the responsible technical committee, 1 which you may attend.
8 It is recommended that for each new supply of the solvent a blank should be run
on an asphalt of known properties.
Trang 4a speed calculated to produce a centrifugal force of not less
than 3000 times gravity
9.3 Concentrate the solution to about 200 ml by any primary
distillation operation using a flask large enough to hold all the
solution from the extraction Transfer the residue from the
primary distillation flask, using several washes of solvent to
rinse all of the residue into the 250-ml distillation flask
Assemble the apparatus as shown inFig 2, except position the
bottom of the aeration tube above the surface of the solution
Continue distillation until the temperature reaches 135°C
(275°F), at which time lower the aeration tube so that the bulb
is in contact with the bottom of the flask, and introduce carbon
dioxide gas at a low rate (approximately 100 ml/min) to
provide agitation and prevent foaming If foaming or bumping
occurs, introduce carbon dioxide intermittently at the
begin-ning of the distillation at a rate of 100 ml/min to prevent this
When the temperature reaches 157 to 160°C (315 to 320°F),
increase the carbon dioxide gas flow to approximately 900
mL/min Maintain this gas flow rate for 10 min while also
maintaining the temperature of the residue in the flask at 160 to
166°C (320 to 330°F) If, after 10 min, dripping of condensed
solvent from the delivery tube is still occurring, maintain the
gas flow and temperature until 5 min after the dripping ceases
in order to flush solvent vapors from the flask In no case shall
the time of flow of carbon dioxide gas be less than 15 min At
the end of this period, discontinue gas flow and heat
9.3.1 Alternative Procedure—Assemble the apparatus as
shown inFig 2with the separatory funnel in the thermometer
hole in the cork (It may be advantageous to insert the
separatory funnel in a separate hole drilled in the cork stopper.)
Raise the aeration tube so that the bulb is above the surface of
the solution Fill the separatory funnel with the centrifuged
solution and open the stopcock to fill the flask approximately
one half full of solvent mixture Apply low heat to the flask and
start distillation Adjust the funnel stopcock to introduce fresh
solvent at a rate that will keep the flask approximately one half
full during distillation, adding additional solvent mixture to the
funnel until all solvent has been introduced into the distillation
flask Wash the solvent mixture container and funnel with fresh
solvent to transfer all asphalt into the distillation flask
Con-tinue distillation until the temperature reaches 135°C (275°F),
at which time lower the aeration tube so that the bulb is in
contact with the bottom of the flask and introduce carbon
dioxide gas at a low rate (approximately 100 ml/min) to
provide agitation and prevent foaming If foaming or bumping
occurs, introduce carbon dioxide intermittently at the
begin-ning of the distillation at a rate of 100 ml/min to prevent this
When the temperature reaches 157 to 160°C (315 to 320°F),
increase the carbon dioxide gas flow to approximately 900
mL/min Maintain this gas flow rate for 10 min while also
maintaining the temperature of the residue in the flask at 160 to
166°C (320 to 330°F) If, after 10 min, dripping of condensed
solvent from the delivery tube is still occurring, maintain the
gas flow and temperature until 5 min after the dripping ceases
in order to flush solvent vapors from the flask In no case shall
the time of flow of carbon dioxide gas be less than 15 min At
the end of this period, discontinue the gas flow and heat
9.4 If the residue in the flask is highly viscous at 163°C (325°F), so that dispersion of the carbon dioxide in the residue
is restricted and the recovered asphalt is expected to have a penetration at 25°C (77°F) of less than 30, maintain the carbon dioxide gas flow and temperature for 20 to 22 min
9.5 The recovered asphalt can be heated to reliquefy and portions taken for penetration, softening point, ductility, ash content, and kinematic and absolute viscosity determinations
as required Ash content determinations shall be conducted on all recovered bitumens in accordance with Test Methods D2939 and reported with other test data on the recovered asphalt Ash contents of recovered asphalts greater than 1 % may affect the accuracy of the penetration, ductility, softening point, or viscosity tests
N OTE 1—Determination of the weight of asphalt recovered serves as a check to assure that all of the solvent has been removed when this weight
is compared with the weight of asphalt extracted as determined by Test Methods D2172 The weight of the recovered asphalt should be corrected for the ash content determined.
10 Precision and Bias
10.1 Precision—Data from the AMRL9proficiency sample database from 1974 to 1992 was analyzed to develop estimates
of test precision.10The results of the analysis are summarized below The grades of asphalt binders included in the analysis consisted of AC-5, AC-10, AC-15, AC-20, AC-30, AC-40, AR-2000, and AR-4000 The precision estimates provided apply to unaged asphalt binder having physical test properties within the following ranges:
Penetration at 25°C (77°F) 29 to 181 Kinematic viscosity at 135°C (275°F), cSt 200 to 720 Viscosity at 60°C (140°F), P 520 to 5320
10.1.1 Single-Operator Precision—The figures given in
Column 2 are the coefficients of variation that have been found
to be appropriate for the tests and conditions described in Column 1 When performed by the same operator on the same sample in the same laboratory using the same apparatus, the difference in the results of two properly conducted tests, expressed as a percent of their mean, shall not exceed the figures given in Column 3
Test Index
Coefficient of Variation (percent of mean) 12
Acceptable Range of Two Results (percent of mean) 12
Single-Operator Precision:
Penetration at 25°C (77°F)
Kinematic viscosity at 135°C (275°F), cSt
Viscosity at 60°C (140°F), P
10.1.2 Multilaboratory Precision—The figures given in
Column 2 are the coefficients of variation that have been found
to be appropriate for the tests and conditions described in Column 1 When performed by different operators in the different laboratories, the difference in the results of two
9 These numbers represent, respectively, the (1s %) and (d2s %) limits as described in ASTM Practice C670
10 Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D04-1008.
Trang 5properly conducted tests, expressed as a percent of their mean,
shall not exceed the figures given in Column 3
Test Index
Coefficient of Variation (percent of mean) 12
Acceptable Range of Two Results (percent of mean) 12
Multilaboratory Precision:
Penetration at 25°C
(77°F)
Kinematic viscosity at
135°C (275°F), cSt
Viscosity at 60°C
(140°F), P
10.2 Bias—Since there is no data at this time to prepare a
bias statement, no statement on bias is made
11 Keywords
11.1 asphalt; bituminous mixture; distillation; solution
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